CN105776269A - Micro-powder aluminum hydroxide preparation method and device and micro-powder aluminum hydroxide - Google Patents
Micro-powder aluminum hydroxide preparation method and device and micro-powder aluminum hydroxide Download PDFInfo
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- CN105776269A CN105776269A CN201610171923.2A CN201610171923A CN105776269A CN 105776269 A CN105776269 A CN 105776269A CN 201610171923 A CN201610171923 A CN 201610171923A CN 105776269 A CN105776269 A CN 105776269A
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- aluminium hydroxide
- intermediate product
- sodium aluminate
- aluminate solution
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- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 56
- 239000000843 powder Substances 0.000 title abstract 7
- 239000013067 intermediate product Substances 0.000 claims abstract description 64
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 62
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 29
- 239000013078 crystal Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010521 absorption reaction Methods 0.000 claims abstract description 8
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 98
- 238000000034 method Methods 0.000 claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000012065 filter cake Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 10
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 9
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 239000000470 constituent Substances 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- 238000004131 Bayer process Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 10
- 238000009826 distribution Methods 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract 2
- 239000012535 impurity Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000000779 smoke Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012757 flame retardant agent Substances 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000007701 flash-distillation Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
- C01F7/142—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent with carbon dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a micro-powder aluminum hydroxide preparation method and device and micro-powder aluminum hydroxide. The preparation method comprises the steps of adding aluminum hydroxide seed crystals obtained through carbonation decomposition of a sodium aluminate solution into the sodium aluminate solution to perform variable-temperature seed decomposition to obtain decomposition slurry; removing iron in the decomposition slurry to obtain a first intermediate product; washing the first intermediate product to depolymerize the first intermediate product to obtain a second intermediate product; removing water in the second intermediate product to obtain a third intermediate product; scattering and grading the third intermediate product to obtain micro-powder aluminum hydroxide. The preparation device comprises a decomposition tank, an iron removing device, a first washing device, a depolymerization device, a water removing device, and a scattering and grading device. The micro-powder aluminum hydroxide is prepared by using the preparation device according to the preparation method, such that the grain distribution of the micro-powder aluminum hydroxide product with a median particle diameter of 1mu m is even, the oil absorption is reduced to 30mL/100g to 35mL/100g, the impurity content of the obtained product is low, the whiteness is high and the product quality is stable.
Description
Technical field
The present invention relates to aluminium hydroxide technical field, particularly relate to a kind of aluminium hydroxide micropowder preparation method and equipment, this aluminium hydroxide micropowder.
Background technology
Aluminium hydroxide micropowder is a kind of environmental-protection flame-retardant filler, is mainly used in the industries such as electric cable material with low smoke and halogen free, composite insulator, copper-clad plate, expanded material.In recent years, along with national environmental protection policy is constantly upgraded and industry restructuring, the development of the new industry such as domestic composite insulator, electric wire, electronic apparatus, high ferro, 3G/4G network is swift and violent, and the Low-smoke halogen-free environment-friendlyflame-retardant flame-retardant agent market demand is vigorous.Aluminium hydroxide micropowder is as the Low-smoke halogen-free environment-friendlyflame-retardant flame-retardant agent of function admirable, also the track of high speed development has been striden into therewith, it itself is not only a kind of functional material, and the exploitation for new material provides wide application prospect, has extremely important effect in the many fields of national economy.
At present, the production of aluminium hydroxide micropowder is commonly used adds crystal seed stirring decomposition preparation at a certain temperature in sodium aluminate solution, and this kind of equipment is simple, and production process is prone to grasp.But, the crystal seed that existing process conditions adopt is levigate aluminium hydroxide mostly or reacts, by neutralizing, the amorphous state seed liquor obtained, when not controlling catabolic process temperature, the aluminium hydroxide micropowder Granularity Distribution of preparation is wider, oil absorbency is higher, sodium oxide content is higher, in the use procedure of user, to go out processing characteristics bad for common manifestation, awaits further improvement, raising.
Summary of the invention
In view of this, the present invention provides a kind of aluminium hydroxide micropowder preparation method and equipment, this aluminium hydroxide micropowder, applies this Preparation equipment, grows perfect with the aluminium hydroxide micropowder crystallization that this preparation method prepares, and purity is higher, thus more suitable for practicality.
In order to reach above-mentioned first purpose, the technical scheme of aluminium hydroxide micropowder preparation method provided by the invention is as follows:
Aluminium hydroxide micropowder preparation method provided by the invention comprises the following steps:
Add in sodium aluminate solution and decompose, by sodium aluminate solution carbonation, the aluminium hydroxide crystal seed obtained, carry out alternating temperature kind decomposition, obtain decomposing slip；
Remove the ferrum in described decomposition slurry, obtain the first intermediate product；
After washing described first intermediate product so that it is depolymerization, obtain the second intermediate product；
Remove the moisture in the second intermediate product, obtain the 3rd intermediate product；
Break up and the 3rd intermediate product described in classification, prepare described aluminium hydroxide micropowder.
Aluminium hydroxide micropowder preparation method provided by the invention also can be applied to the following technical measures to achieve further.
As preferably, described sodium aluminate solution is to adopt sintering process, or, Bayer process, or, after the aluminium hydroxide molten method of weight, obtaining through fine straining, the span of described sodium aluminate solution α K is 1.4～1.7, in described sodium aluminate solution, Na2The span of O content is 90g/L～150g/L, and in described sodium aluminate solution, the span of floating material content is≤0.020g/L.
As preferably, adding in sodium aluminate solution and decompose, by sodium aluminate solution carbonation, the aluminium hydroxide crystal seed obtained, carry out alternating temperature kind decomposition, when obtaining decomposing slip,
In sodium aluminate solution, add that to decompose, by sodium aluminate solution carbonation, the span that opportunity is sodium aluminate solution liquid temp of aluminium hydroxide crystal seed obtained be 50 DEG C～75 DEG C；
After decomposing, by sodium aluminate solution carbonation, the aluminium hydroxide crystal seed 4h～10h obtained described in adding, control decomposer temperature and be reduced to 40 DEG C～60 DEG C；
55 DEG C～70 DEG C are lifted temperature to before described decomposition stock discharge.
As preferably, removing the ferrum in described decomposition slurry, when obtaining the first intermediate product,
The method removing the ferrum in described decomposition slurry is wet method；
After washing described first intermediate product so that it is depolymerization, when obtaining the second intermediate product, described depolymerization method is wet method.
As preferably, the span of the described granularity D50 being decomposed the aluminium hydroxide crystal seed obtained by sodium aluminate solution carbonation is 2.5 μm～4.5 μm, the span of seed count is 150g/L～300g/L, and addition is the 0.5%～5% of sodium aluminate solution quality.
As preferably, adding and decompose, by sodium aluminate solution carbonation, the aluminium hydroxide crystal seed obtained, carry out alternating temperature kind decomposition in sodium aluminate solution, when obtaining decomposing slip, the span of resolution ratio is 50%～55%.
As preferably, the moisture in described removing the second intermediate product, when obtaining three intermediate products, including described second intermediate product carries out solid-liquor separation washing, reduces filter cake moisture, obtains the filter cake after dehydration, weight/mass percentage composition≤30% of water in described filter cake.
In order to reach above-mentioned second purpose, the technical scheme of aluminium hydroxide micropowder Preparation equipment provided by the invention is as follows:
Aluminium hydroxide micropowder Preparation equipment provided by the invention includes decomposer, deironing apparatus, the first wash mill, depolymerizer, water trap, breaks up and grading plant,
Described decomposer, for housing sodium aluminate solution and being decomposed the aluminium hydroxide crystal seed obtained by sodium aluminate solution carbonation, makes described sodium aluminate solution carry out alternating temperature kind decomposition, obtains decomposing slurry；
Described deironing apparatus, for removing the ferrum in described decomposition slurry, obtains the first intermediate product；
Described first wash mill is used for washing described first intermediate product；
Described depolymerizer through the first intermediate product of washing, obtains the second intermediate product described in depolymerization；
Described water trap, for removing the moisture in described second intermediate product, obtains described 3rd intermediate product；
Described break up with grading plant for break up and classification described in the 3rd intermediate product, prepare described aluminium hydroxide micropowder.
Aluminium hydroxide micropowder Preparation equipment provided by the invention also can be applied to the following technical measures to achieve further.
As preferably, described aluminium hydroxide micropowder Preparation equipment also includes temperature-adjusting device, and described temperature-adjusting device is for being adjusted the temperature of described decomposer.
In order to reach above-mentioned 3rd purpose, the technical scheme of aluminium hydroxide micropowder provided by the invention is as follows:
Aluminium hydroxide micropowder provided by the invention applies aluminium hydroxide micropowder Preparation equipment provided by the invention, prepares with aluminium hydroxide micropowder preparation method provided by the invention,
The parameter of described aluminium hydroxide micropowder is as follows:
Each constituent mass percentage composition is respectively as follows: Fe2O3:≤0.008%, Na2O:0.083%～0.100%, Na2O(s): 0.006%～0.014%, SiO2:≤0.01%；
Whiteness: 96.9%～98.8%；
D50:1.03 μm～1.35 μm；
Attached water: 0.173%～0.234%；
Oil absorption: 30～35；
D90:1.56 μm～2.65 μm.
Apply aluminium hydroxide micropowder Preparation equipment provided by the invention, be respectively as follows: Fe with each constituent mass percentage composition of aluminium hydroxide micropowder that aluminium hydroxide micropowder preparation method provided by the invention prepares2O3:≤0.008%, Na2O:0.083%～0.100%, Na2O(s): 0.006%～0.014%, SiO2:≤0.01%；Whiteness: 96.9%～98.8%；D50:1.03 μm～1.35 μm；Attached water: 0.173%～0.234%；Oil absorption: 30～35；D90:1.56 μm～1.35 μm, and, constant product quality.
Accompanying drawing explanation
By reading hereafter detailed description of the preferred embodiment, various other advantage and benefit those of ordinary skill in the art be will be clear from understanding.Accompanying drawing is only for illustrating the purpose of preferred implementation, and is not considered as limitation of the present invention.And in whole accompanying drawing, it is denoted by the same reference numerals identical parts.In the accompanying drawings:
Accompanying drawing 1 is the flow chart of steps of aluminium hydroxide micropowder preparation method provided by the invention；
Accompanying drawing 2 is the annexation schematic diagram of aluminium hydroxide micropowder preparation facilities provided by the invention；
Accompanying drawing 3 is the electromicroscopic photograph of aluminium hydroxide micropowder provided by the invention.
Detailed description of the invention
The present invention solves prior art Problems existing, a kind of aluminium hydroxide micropowder preparation method and equipment, this aluminium hydroxide micropowder are provided, apply this Preparation equipment, grow perfect with the aluminium hydroxide micropowder crystallization that this preparation method prepares, purity is higher, thus more suitable for practicality.
For further setting forth that the present invention reaches technological means and effect that predetermined goal of the invention is taked, below in conjunction with accompanying drawing and preferred embodiment, to the aluminium hydroxide micropowder preparation method proposed according to the present invention and equipment, this aluminium hydroxide micropowder, its detailed description of the invention, structure, feature and effect thereof, describe in detail as after.In the following description, what different " embodiments " or " embodiment " referred to is not necessarily same embodiment.Additionally, special characteristic in one or more embodiment, structure or feature can be combined by any suitable form.
The terms "and/or", is only a kind of incidence relation describing affiliated partner, and expression can exist three kinds of relations, such as, A and/or B, concrete is interpreted as: can include A and B simultaneously, can individualism A, it is also possible to individualism B, it is possible to possess above-mentioned three kinds of any one situations.
Embodiment 1
Referring to accompanying drawing 1, the aluminium hydroxide micropowder preparation method that the embodiment of the present invention 1 provides comprises the following steps:
Step S1: add in sodium aluminate solution and decompose, by sodium aluminate solution carbonation, the aluminium hydroxide crystal seed obtained, carry out alternating temperature kind decomposition, obtains decomposing slip；
Step S2: remove the ferrum decomposed in slurry, obtain the first intermediate product；
Step S3: after washing the first intermediate product so that it is depolymerization, obtains the second intermediate product；
Step S4: remove the moisture in the second intermediate product, obtains the 3rd intermediate product；
Step S5: break up and classification the 3rd intermediate product, prepares aluminium hydroxide micropowder.
The each constituent mass percentage composition of aluminium hydroxide micropowder that the aluminium hydroxide micropowder preparation method provided with the embodiment of the present invention 1 prepares is respectively as follows: Fe2O3: 0.008%, Na2O:0.096%, Na2O(s): 0.01%, SiO2: 0.01；Whiteness: 98.3%；D50:1.23 μm；Attached water: 0.234%；Oil absorption: 3633；D90:1.99 μm, and, constant product quality.
Wherein, sodium aluminate solution is to adopt sintering process, or, Bayer process, or, after the aluminium hydroxide molten method of weight, obtaining through fine straining, sodium aluminate solution α K is 1.4, in sodium aluminate solution, Na2O content is 90g/L, and in sodium aluminate solution, the span of floating material content is≤0.0.010g/L.
Wherein, add in sodium aluminate solution and decompose, by sodium aluminate solution carbonation, the aluminium hydroxide crystal seed obtained, carry out alternating temperature kind decomposition, when obtaining decomposing slip, the span that opportunity is sodium aluminate solution liquid temp adding the aluminium hydroxide crystal seed that β phase is obtained by sodium aluminate solution carbonation decomposition in sodium aluminate solution is 60 DEG C；After adding aluminium hydroxide crystal seed 4h, control decomposer temperature and be reduced to 50 DEG C；60 DEG C are lifted temperature to before decomposing stock discharge.
Wherein, removing the ferrum decomposed in slurry, when obtaining the first intermediate product, the method removing the ferrum decomposed in slurry is wet method；After washing the first intermediate product so that it is depolymerization, when obtaining the second intermediate product, depolymerization method is wet method.
Wherein, the span being decomposed the granularity D50 of aluminium hydroxide crystal seed obtained by sodium aluminate solution carbonation is 2.5 μm, and the span of seed count is 150g/L, and addition is the 1% of sodium aluminate solution quality.
Wherein, adding and decompose, by sodium aluminate solution carbonation, the aluminium hydroxide crystal seed obtained, carry out alternating temperature kind decomposition in sodium aluminate solution, when obtaining decomposing slip, the span of resolution ratio is 52%.
Wherein, removing the moisture in the second intermediate product, when obtaining three intermediate products, including the second intermediate product carries out solid-liquor separation washing, reduce filter cake moisture, obtain the filter cake after dehydration, in filter cake, the weight/mass percentage composition of water is 28%.
In the present embodiment, depolymerization is to adopt wet milk to realize；Afterwards, adopting vertical type blotter press to carry out solid-liquid separation washing, reduce filter cake moisture, filter cake enters spin flash dryer after dehydration, drying air intake and has to pass through purification, in order to avoid causing in drying course, product being polluted.In this way, it is possible to improve the stability of product.
Embodiment 2
Referring to accompanying drawing 2, the aluminium hydroxide micropowder Preparation equipment that the embodiment of the present invention 2 provides includes decomposer, deironing apparatus, the first wash mill, depolymerizer, water trap, breaks up and grading plant, decomposer is for housing sodium aluminate solution and being decomposed the aluminium hydroxide crystal seed obtained by sodium aluminate solution carbonation, make sodium aluminate solution carry out alternating temperature kind decomposition, obtain decomposing slurry；Deironing apparatus is used for away decomposing the ferrum in slurry, obtains the first intermediate product；First wash mill is used for washing the first intermediate product；Depolymerizer through the first intermediate product washed, obtains the second intermediate product for depolymerization；Water trap, for removing the moisture in the second intermediate product, obtains the 3rd intermediate product；Break up with grading plant for breaing up and classification the 3rd intermediate product, prepare aluminium hydroxide micropowder.
Apply aluminium hydroxide micropowder Preparation equipment provided by the invention, be respectively as follows: Fe with each constituent mass percentage composition of aluminium hydroxide micropowder that aluminium hydroxide micropowder preparation method provided by the invention prepares2O3: 0.008%, Na2O:0.091%, Na2O(s): 0.008%, SiO2: 0.01%；Whiteness: 97.2%；D50:1.18 μm；Attached water: 0.213%；Oil absorption: 30；D90:1.89 μm, and, constant product quality.
In the present embodiment, depolymerizer is wet milk.
In the present embodiment, water trap includes:
Vertical type blotter press, is used for carrying out solid-liquid separation washing, thus reducing filter cake moisture；
Rotary flash distillation dryer, for being dried the filter cake through dehydration；
Dry wind purifying device, for drying air intake is purified, thus avoiding aluminium hydroxide micropowder to receive pollution, wherein, drying wind purifying device and can select purifier of the prior art, such as ultrafiltration, microfiltration, reverse osmosis unit etc..
Additionally, this Preparation equipment can also include packing device, for aluminium hydroxide micropowder product is packed.
Wherein, aluminium hydroxide micropowder Preparation equipment also includes temperature-adjusting device, temperature-adjusting device is for being adjusted the temperature of decomposer so that, in sodium aluminate solution, add that to decompose opportunity of the aluminium hydroxide crystal seed obtained by sodium aluminate solution carbonation be sodium aluminate solution liquid temp be 60 DEG C；After adding aluminium hydroxide crystal seed 4h, control decomposer temperature and be reduced to 50 DEG C；60 DEG C are lifted temperature to before decomposing stock discharge.
In the present embodiment, temperature-adjusting device can be arranged on the control panel of decomposer；This temperature-adjusting device can also be arranged on long-range PC or handheld terminal, and now, this temperature-adjusting device can also be fabricated to an APP and be installed on operator's mobile phone or pad.In addition, Threshold Alerts device can also be set, once any marginal value in decomposer temperature triggered said temperature threshold value, namely this Threshold Alerts device reports to the police, signal lights, buzzer, qq message, note, wechat message, speech message etc. can be passed through by Temperature numerical teaching process personnel, in order to operator take corresponding actions at any time.
Embodiment 3
Referring to accompanying drawing 3, the aluminium hydroxide micropowder Preparation equipment that the aluminium hydroxide micropowder application embodiment of the present invention 2 that the embodiment of the present invention 3 provides provides, preparing with the aluminium hydroxide micropowder preparation method that the embodiment of the present invention 1 provides, the parameter of aluminium hydroxide micropowder is as follows: each constituent mass percentage composition is respectively as follows: Fe2O3: 0.008%, Na2O:0.086%, Na2O(s): 0.009%, SiO2: 0.01%；Whiteness: 98.2%；D50:1.26 μm；Attached water: 0.209%；Oil absorption: 33；D90:1.1.97 μm.
The preparation method of the micropowder hydrogen aluminum of the embodiment of the present invention 4～20 application is identical with the preparation method step of the micropowder hydrogen aluminum that the embodiment of the present invention 1 or 2 is applied, but operating parameter, result parameter are different；The Preparation equipment of the modified micropowder hydrogen aluminum that the Preparation equipment of the micropowder hydrogen aluminum of the embodiment of the present invention 4～20 application is applied with the embodiment of the present invention 1 or 2 is identical, but operating parameter, result parameter are different.
Table 1 embodiment 4～20 operating parameter
Continued 1 embodiment 4～21 result parameter
According to the result shown in continued 1, it is known that, apply aluminium hydroxide micropowder Preparation equipment provided by the invention, be respectively as follows: Fe with each constituent mass percentage composition of aluminium hydroxide micropowder that aluminium hydroxide micropowder preparation method provided by the invention prepares2O3:≤0.008%, Na2O:0.083%～0.100%, Na2O(s): 0.006%～0.014%, SiO2:≤0.01%；Whiteness: 96.9%～98.8%；D50:1.03 μm～1.35 μm；Attached water: 0.173%～0.234%；Oil absorption: 30～35；D90:1.56 μm～1.35 μm, and, constant product quality.
Although preferred embodiments of the present invention have been described, but those skilled in the art are once know basic creative concept, then these embodiments can be made other change and amendment.So, claims are intended to be construed to include preferred embodiment and fall into all changes and the amendment of the scope of the invention.
Obviously, the present invention can be carried out various change and modification without deviating from the spirit and scope of the present invention by those skilled in the art.So, if these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (10)
1. an aluminium hydroxide micropowder preparation method, it is characterised in that comprise the following steps:
Add in sodium aluminate solution and decompose, by sodium aluminate solution carbonation, the aluminium hydroxide crystal seed obtained, carry out alternating temperature kind decomposition, obtain decomposing slip；
Remove the ferrum in described decomposition slurry, obtain the first intermediate product；
After washing described first intermediate product so that it is depolymerization, obtain the second intermediate product；
Remove the moisture in the second intermediate product, obtain the 3rd intermediate product；
Break up and the 3rd intermediate product described in classification, prepare described aluminium hydroxide micropowder.
2. aluminium hydroxide micropowder preparation method according to claim 1, it is characterized in that, described sodium aluminate solution is to adopt sintering process, or, Bayer process, or, after the aluminium hydroxide molten method of weight, obtaining through fine straining, the span of described sodium aluminate solution α K is 1.4～1.7, in described sodium aluminate solution, Na2The span of O content is 90g/L～150g/L, and in described sodium aluminate solution, the span of floating material content is≤0.020g/L.
3. aluminium hydroxide micropowder preparation method according to claim 1, it is characterised in that add in sodium aluminate solution and decompose, by sodium aluminate solution carbonation, the aluminium hydroxide crystal seed obtained, carry out alternating temperature kind decomposition, when obtaining decomposing slip
In sodium aluminate solution, add that to decompose, by sodium aluminate solution carbonation, the span that opportunity is sodium aluminate solution liquid temp of aluminium hydroxide crystal seed obtained be 50 DEG C～75 DEG C；
After decomposing, by sodium aluminate solution carbonation, the aluminium hydroxide crystal seed 4h～10h obtained described in adding, control decomposer temperature and be reduced to 40 DEG C～60 DEG C；
55 DEG C～70 DEG C are lifted temperature to before described decomposition stock discharge.
4. aluminium hydroxide micropowder preparation method according to claim 1, it is characterised in that remove the ferrum in described decomposition slurry, when obtaining the first intermediate product,
The method removing the ferrum in described decomposition slurry is wet method；
After washing described first intermediate product so that it is depolymerization, when obtaining the second intermediate product, described depolymerization method is wet method.
5. aluminium hydroxide micropowder preparation method according to claim 1, it is characterized in that, the span of the described granularity D50 being decomposed the aluminium hydroxide crystal seed obtained by sodium aluminate solution carbonation is 2.5 μm～4.5 μm, the span of seed count is 150g/L～300g/L, and addition is the 0.5%～5% of sodium aluminate solution quality.
6. aluminium hydroxide micropowder preparation method according to claim 1, it is characterized in that, add in sodium aluminate solution and decompose, by sodium aluminate solution carbonation, the aluminium hydroxide crystal seed obtained, carry out alternating temperature kind decomposition, when obtaining decomposing slip, the span of resolution ratio is 50%～55%.
7. aluminium hydroxide micropowder preparation method according to claim 1, it is characterized in that, moisture in described removing the second intermediate product, when obtaining three intermediate products, solid-liquor separation washing is carried out including to described second intermediate product, reduce filter cake moisture, obtain the filter cake after dehydration, weight/mass percentage composition≤30% of water in described filter cake.
8. an aluminium hydroxide micropowder Preparation equipment, it is characterised in that include decomposer, deironing apparatus, the first wash mill, depolymerizer, water trap, break up and grading plant,
Described decomposer, for housing sodium aluminate solution and being decomposed the aluminium hydroxide crystal seed obtained by sodium aluminate solution carbonation, makes described sodium aluminate solution carry out alternating temperature kind decomposition, obtains decomposing slurry；
Described deironing apparatus, for removing the ferrum in described decomposition slurry, obtains the first intermediate product；
Described first wash mill is used for washing described first intermediate product；
Described depolymerizer through the first intermediate product of washing, obtains the second intermediate product described in depolymerization；
Described water trap, for removing the moisture in described second intermediate product, obtains described 3rd intermediate product；
Described break up with grading plant for break up and classification described in the 3rd intermediate product, prepare described aluminium hydroxide micropowder.
9. aluminium hydroxide micropowder Preparation equipment according to claim 8, it is characterised in that also include temperature-adjusting device, described temperature-adjusting device is for being adjusted the temperature of described decomposer.
10. an aluminium hydroxide micropowder, it is characterised in that application aluminium hydroxide micropowder Preparation equipment described in claim 8 or 9, prepares with described aluminium hydroxide micropowder preparation method arbitrary in claim 1～7,
The parameter of described aluminium hydroxide micropowder is as follows:
Each constituent mass percentage composition is respectively as follows: Fe2O3:≤0.008%, Na2O:0.083%～0.100%, Na2O(s): 0.006%～0.014%, SiO2:≤0.01%；
Whiteness: 96.9%～98.8%；
D50:1.03 μm～1.35 μm；
Attached water: 0.173%～0.234%；
Oil absorption: 30～35；
D90:1.56 μm～2.65 μm.
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| CN107265487A (en) * | 2017-06-15 | 2017-10-20 | 郑州中绿环保新材料有限公司 | A kind of method that use solid sodium aluminate produces special aluminium hydroxide product |
| CN108569714A (en) * | 2018-04-17 | 2018-09-25 | 郝亚明 | It improves and decomposes aluminium hydroxide micro powder resolution ratio method |
| CN109368674A (en) * | 2018-12-26 | 2019-02-22 | 贵州博汇联润铝业有限公司 | A kind of high temperature resistant low-sodium aluminum hydroxide micro mist preparation method |
| CN109422285A (en) * | 2017-08-30 | 2019-03-05 | 洛阳中超新材料股份有限公司 | Low oil factor aluminium hydroxide and its preparation method and application |
| CN109626406A (en) * | 2018-12-10 | 2019-04-16 | 贵州博汇联润铝业有限公司 | A kind of ultra-fine ultrawhite aluminum hydroxide micro mist preparation method |
| CN110655095A (en) * | 2019-10-16 | 2020-01-07 | 淄博鹏丰铝业有限公司 | Preparation method of low-oil-absorption-value aluminum hydroxide micropowder flame retardant |
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| CN107265487A (en) * | 2017-06-15 | 2017-10-20 | 郑州中绿环保新材料有限公司 | A kind of method that use solid sodium aluminate produces special aluminium hydroxide product |
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| CN109422285A (en) * | 2017-08-30 | 2019-03-05 | 洛阳中超新材料股份有限公司 | Low oil factor aluminium hydroxide and its preparation method and application |
| CN108569714A (en) * | 2018-04-17 | 2018-09-25 | 郝亚明 | It improves and decomposes aluminium hydroxide micro powder resolution ratio method |
| CN109626406A (en) * | 2018-12-10 | 2019-04-16 | 贵州博汇联润铝业有限公司 | A kind of ultra-fine ultrawhite aluminum hydroxide micro mist preparation method |
| CN109626406B (en) * | 2018-12-10 | 2021-03-16 | 贵州博汇联润铝业有限公司 | Preparation method of superfine ultra-white aluminum hydroxide micro powder |
| CN109368674A (en) * | 2018-12-26 | 2019-02-22 | 贵州博汇联润铝业有限公司 | A kind of high temperature resistant low-sodium aluminum hydroxide micro mist preparation method |
| CN110655095A (en) * | 2019-10-16 | 2020-01-07 | 淄博鹏丰铝业有限公司 | Preparation method of low-oil-absorption-value aluminum hydroxide micropowder flame retardant |
| CN110655095B (en) * | 2019-10-16 | 2021-11-30 | 淄博鹏丰新材料科技有限公司 | Preparation method of low-oil-absorption-value aluminum hydroxide micropowder flame retardant |
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